Inorganic Experiments Woollins.pdf
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There are not a whole lot of manuals aimed atsenior-levelundergraduate laboratory courses in inorganicchemistry. Only fourwere published in the 90s: Szafran, Pike,and Singhs MicroscaleInorganic Chemistry (1), the 3rd edi-tion of Angelicis classicSynthesis and Technique in InorganicChemistry updated by Girolamiand Rauchfuss (2), Tanakaand Suibs Experimental Methods inInorganic Chemistry (3),and the 1st edition of Woollins InorganicExperiments (4).While this shortage is arguably a consequence ofthe tendencyby many instructors to simply design such courses basedonpersonal experience or experimental procedures reported inthisJournal or in serials such as Inorganic Syntheses, it is clearthatthe need for innovative, stimulating experiments andtextsremains.
The first edition of Inorganic Experiments has been com-pletelyrevised and enlarged (more enlarged than revised, Iwould say) andit continues to exhibit several features thatdistinguish it fromits current market competitors. It is nowa collection of almost 90experiments written by a group of63 international contributors(about half of whom are in theUK). While this is not necessarily anadvantage over bookswritten by two or three authors, it doesreflect an effort todraw experiments from individuals with adiversity of back-grounds and research interests. Perhaps moreimportantly, itis still the only inorganic laboratory manual thatcontainsseparate sections for introductory, intermediate, andadvancedexperiments. Almost 100 additional pages and 24 newex-periments (eight in each section) have been added to thisnewedition, thus giving instructors even more options to choosefromfor selected topics or to adjust the course to time orenrollmentconstraints.
The 2nd edition of Inorganic Experiments starts with abriefintroduction to the expository (skills-oriented) and in-vestigative(discovery-oriented) approaches to laboratory in-struction (5).Since much has been written about the benefitsof inquiry-based ordiscovery-oriented laboratory experiences(6), it is fortunate thatWoollins book follows this model inmost of its experiments. Chapter2 (Introductory Experi-ments) deals with the preparation of varioussimple inorganiccompounds and coordination complexes, includingiron(III)oxalate complexes, interhalogen compounds, andsiloxanepolymers. Even straightforward experiments have agoodpedagogic value when presented in the right context. Forex-ample, the preparation of copper(I) iodide from its elements
Chapter 3 contains 31 experiments of intermediate com-plexity.While classic coordination chemistry is still repre-sented by thesyntheses of a number of acetylacetonate,dinitrogen, and phosphinecomplexes, organometallic chem-istry is the predominant theme inthis chapter. From thesyntheses of ferrocene and some of itsderivatives to the prepa-ration of a tungsten alkylidyne complex,many proceduresin this chapter also require the handling ofair-sensitive com-pounds (e.g., Grignard and organolithiumreagents). Amongmy favorite experiments are the synthesis andmultinuclearNMR characterization of trans-PtHCl(PPh3)2 and thestudyof the paramagnetism of iron(III) dithiocarbamate complexesinsolution by the Evans method.
Even more challenging are the 33 experiments includedin Chapter4, some of which rely on the use of more special-ized techniques(e.g., electron paramagnetic resonance (EPR)spectroscopy) or moreesoteric reaction conditions (e.g., liq-uid ammonia as a solvent).In fact, I suspect that a few ofthe experiments in this chapterwill probably be too com-plex to implement in most undergraduatesettings even if thenecessary equipment, a generous budget, andqualified in-structors are available. A case in point is thesynthesis of thefascinating 17-electron hexacarbonyl V(CO)6, whichstartswith the preparation of a vanadate precursor in anautoclavecharged with vanadium trichloride, sodium sand, and 200atmof CO. Not precisely your everyday synthesis of copper(I)iodide!But there is no question that many of these advancedexperiments areaimed at bringing contemporary researchtopics to the undergraduatearena: the synthesis of ahigh-valent manganese imido complex, theinvestigation ofmetal-containing liquid crystals, and thecoordination chem-istry of organic free radicals are just threeadditional examples.
The book has been for the most part carefully producedand isnicely organized, including a five-page subject index,and Ivedetected only a handful of typographical errors (e.g.,piperideneinstead of piperidine [p 144]) or mistaken ref-erences (e.g., theyear of publication of the fourth referencein p 198 is 1999 not1998). However, as is often the casewith edited monographs, thethoroughness or style of theexperimental write-ups is not uniform.For example, not allthe experiments contain a list of questions orexercises forfurther consideration and only a few includesuggestions forthe preparation of reports. Similarly, whereas someexperi-
As much as I personally like this book and believe it is agreatresource for instructors, I cannot say it would be mytop choice asa lab manual for undergraduate students. I stillprefer Girolami,Rauchfuss, and Angelicis book (2), whichhas a shorter list ofexperiments to choose from but, unlikeWoollinss text, has also goodintroductory sections on safety,common laboratory practices, andthe organization of labo-ratory notebooks. In addition, it hasbetter guidelines for re-ports and independent studies and a morecomprehensivebibliography associated with each experiment. In thesamevein, Szafran, Pike, and Singhs manual (1) alsoincorporatesnice individual chapters on safety, equipment,commonmicroscale techniques, spectroscopic methods (almost40pages!), and a more balanced roll of experiments,includingseveral on main group and bioinorganic chemistry. Insum-mary, Inorganic Experiments is an eclectic but veryattractivecompilation of experiments in modern inorganicchemistry,and I highly recommend it to instructors ofundergraduateinorganic laboratory courses and to otherprofessionals witha general interest in synthetic inorganic ororganometallicchemistry.
The aim of the course is to provide students with an in-depth knowledge of the chemical behavior of main groups elements.Objective of the course is also to make students understand the behavior of the elements of the s and p blocks with the help of the periodic table, rationalizing the relationships between groups and periodic trends.The laboratory experiences are designed in order to provide an experimental support to the theoretical part of the course and to develop the manual and mental skills necessary to prepare, characterize and understand the behavior of inorganic compounds.
Laboratory experiences.The experiments were chosen in order to exemplify the concepts discussed in the theoretical part of the course and consist in the synthesis and characterization of compounds of the elements of the main groups, and experiences of their reactivity. An important aspect is the correlation between structure and properties of the studied compounds. 1e1e36bf2d